Hydrogen Sulfide → HCID 178523349, Verbindung

HRID 462922

Reaktionsgleichung

Reaktionsgleichung von HRID 462922
C(N(CC)CC)C.ClC(OCC(C)C)=O.[CH2:16]([O:23][C:24]([NH:26][CH2:27][CH2:28][CH2:29][C:30]([OH:32])=O)=[O:25])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.S.[S:34](=O)(=O)(O)O>C(Cl)Cl>[CH2:16]([O:23][C:24]([NH:26][CH2:27][CH2:28][CH2:29][C:30]([OH:32])=[S:34])=[O:25])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

Komponenten

7

Edukt 5

HCID 402Hydrogen SulfideHCID 1118Sulfuric AcidHCID 8471TriethylamineHCID 211844-(((Benzyloxy)carbonyl)amino)butanoic acidHCID 62365Isobutyl chloroformate

Produkt 1

HCID 178523349HCID 178523349, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

2.2 g (20 mmol) of triethylamine and a solution of 1.4 ml (10 mmol) of isobutyl chloroformate in 20 ml of dry methylene chloride are added dropwise, in succession, to a solution, cooled to -10°, of 2.37 g (10 mmol) of 4-benzyloxycarbonylaminobutyric acid in 50 ml of dry methylene chloride. The reaction mixture is stirred for one hour at -10° and then a strong current of hydrogen sulphide is passed through for 11/2 hours. After warming to room temperature, the mixture is cooled again and acidified with 2N sulphuric acid. The organic phase is separated, dried and concentrated in vacuo. The 4-benzyloxycarbonylaminothiobutyric acid obtained can be used without further purification.

Aufarbeitung

  1. custom2 hours
  2. temperaturethe mixture is cooled again
  3. customThe organic phase is separated
  4. customdried
  5. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-ec1cedfa04a4408385161666c26b9295
Quelldatensatz
uspto-grants-1985_05
Patentnummer
US04518533

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